Water → Methyl 5-(difluoromethoxy)-1-methyl-1H-pyrazole-3-carboxylate

HRID 362651ノート

反応式

HRID 362651 の反応式
[OH:1][C:2]1[N:6]([CH3:7])[N:5]=[C:4]([C:8]([O:10][CH3:11])=[O:9])[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].Cl[CH:19]([F:21])[F:20].O>CN(C)C=O>[F:20][CH:19]([F:21])[O:1][C:2]1[N:6]([CH3:7])[N:5]=[C:4]([C:8]([O:10][CH3:11])=[O:9])[CH:3]=1

参加物

6

反応物 4

HCID 962WaterHCID 6372ChlorodifluoromethaneHCID 11430Potassium CarbonateHCID 178498595HCID 178498595、化合物

生成物 1

HCID 54319416Methyl 5-(difluoromethoxy)-1-methyl-1H-pyrazole-3-carboxylate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
70 °C

実験手順

67.6 g (0.43 mol) 5-Hydroxy-3-methoxycarbonyl-1-methylpyrazole and 299.2 g (2.17 mol) potassium carbonate was dissolved in 1500 ml dimethylformamide and heated to 70° C. At this temperature chlorodifluoromethane was introduced over 2 hours and the mixture stirred at 80° C. for 1.5 hours. The reaction mixture was added to water and extracted 6 times with ethyl acetate. The combined organic phases were washed with saturated aqueous sodium chloride and dried over magnesium sulfate. The reaction solution was concentrated.

後処理

  1. extractionextracted 6 times with ethyl acetate
  2. washThe combined organic phases were washed with saturated aqueous sodium chloride
  3. dry with materialdried over magnesium sulfate
  4. concentrationThe reaction solution was concentrated

出典と根拠

ORDレコード
ord-00d102e2297d4b64bd63ab720ce4305c
出典データセット
uspto-grants-1999_02
特許番号
US05869686

反応ノート

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